PMID- 17177169 OWN - NLM STAT- MEDLINE DCOM- 20070302 LR - 20191210 IS - 0260-437X (Print) IS - 0260-437X (Linking) VI - 27 IP - 1 DP - 2007 Jan-Feb TI - High-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry for the determination of flocoumafen and brodifacoum in whole blood. PG - 18-24 AB - A high-performance liquid chromatographic-tandem mass spectrometric (HPLC-MS-MS) assay was developed and validated to determine quantitatively flocoumafen and brodifacoum in whole blood using warfarin as an internal standard (IS). Liquid-liquid extraction, using ethyl acetate, was used to isolate flocoumafen, brodifacoum and the IS from the biological matrix. Detection was performed on a mass spectrometer by negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The calibration curves were linear (r(2) > 0.998) in the concentration range of 0.1-100.0 ng ml(-1) with a lower limit of quantification of 0.05 ng ml(-1) for flocoumafen, and 0.1 ng ml(-1) for brodifacoum in whole blood. Intra-day and inter-day relative standard deviations (RSDs) were less than 8.0% and 10.8%, respectively. Recoveries of flocoumafen and brodifacoum ranged from 78.0% to 83.7%. This assay can be used to determine trace flocoumafen and brodifacoum in whole blood to investigate suspected poisoning of human and animals. CI - Copyright 2006 John Wiley & Sons, Ltd. FAU - Jin, Mi-Cong AU - Jin MC AD - Ningbo Municipal Center for Disease Control and Prevention, Ningbo 315010, China. jmcjc@nbip.net FAU - OuYang, Xiao-Kun AU - OuYang XK FAU - Chen, Xiao-hong AU - Chen XH LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PT - Validation Study PL - England TA - J Appl Toxicol JT - Journal of applied toxicology : JAT JID - 8109495 RN - 0 (4-Hydroxycoumarins) RN - 0 (Anticoagulants) RN - 2Z80062XQ4 (flocoumafen) RN - 5Q7ZVV76EI (Warfarin) RN - A25P3CP5S7 (bromfenacoum) SB - IM MH - 4-Hydroxycoumarins/*blood/chemistry MH - Anticoagulants/*blood/chemistry MH - Chromatography, High Pressure Liquid/*methods/standards MH - Drug Monitoring/methods MH - Drug Stability MH - Forensic Toxicology/methods MH - Humans MH - Reference Standards MH - Reproducibility of Results MH - Spectrometry, Mass, Electrospray Ionization/*methods/standards MH - Tandem Mass Spectrometry/*methods/standards MH - Warfarin/blood EDAT- 2006/12/21 09:00 MHDA- 2007/03/03 09:00 CRDT- 2006/12/21 09:00 PHST- 2006/12/21 09:00 [pubmed] PHST- 2007/03/03 09:00 [medline] PHST- 2006/12/21 09:00 [entrez] AID - 10.1002/jat.1179 [doi] PST - ppublish SO - J Appl Toxicol. 2007 Jan-Feb;27(1):18-24. doi: 10.1002/jat.1179.